反应详情

Benzyl [2-(dimethylcarbamoyl)ethyl]carbamate (I-139) (0.69 g, 2.76 mmol) was dissolved in tetrahydrofuran (10 ml), and with cooling with ice, sodium hydride (oily, about 55%, 0.15 g, 3.44 mmol) was added, followed by stirring for 10 minutes. Iodomethane (0.26 ml, 4.18 mmol) was added, followed by stirring at room temperature for 18 hours, and water was added. After extraction with ethyl acetate and drying over anhydrous sodium sulfate, the solvent was evaporated away, and the resulting residue was purified by silica gel column chromatography (dichloromethane:methanol=40:1) to obtain a colorless oil (0.63 g, 86%).

1. additionwas added
2. stirringby stirring at room temperature for 18 hours
3. extractionAfter extraction with ethyl acetate
4. dry with materialdrying over anhydrous sodium sulfate
5. customthe solvent was evaporated away
6. customthe resulting residue was purified by silica gel column chromatography (dichloromethane:methanol=40:1)